反応 #2486275

反応方程式

hydrogen

hydrogen

1,5-dinitro naphthalene

water

hydrogen

hydrogen

→

1,5-diamino naphthalene

収率 55.2%

溶媒

aniline

反応条件

後処理

1. 1
   その他was performed at a temperature of about 100° C.
2. 2
   その他the reaction over
3. 3
   その他The catalyst was separated off at about 70° C. by filtration
4. 4
   その他crystallized out
5. 5
   ろ過The crystallate was then filtered off
6. 6
   洗浄washed twice with 50 ml of methanol

実験手順

60 g (0.275 mol) of 1,5-dinitro naphthalene were suspended, in a 700 ml stirrer autoclave, in 340 ml of aniline and treated with 8 g of water-moist, 5% strength catalyst of palladium on activated charcoal, corresponding to 2.8 g of dry catalyst. Hydrogenation was performed at a temperature of about 100° C. and an initial hydrogen pressure of about 10 bars. As soon as the hydrogen pressure dropped to 5 bars, the hydrogen supply was stepped up until the original value of 10 bars was reattained. After 104 minutes the hydrogen uptake was finished and the reaction over. The catalyst was separated off at about 70° C. by filtration and the filtrate cooled to 20° C. whereupon 1,5-diamino naphthalene crystallized out. The crystallate was then filtered off and washed twice with 50 ml of methanol; 24 g of 1,5-diamino naphthalene were obtained with a m.p. of 189°-190° C.

出典